Evaporation is a fundamental process in chemistry and laboratory settings, essential for concentrating solutions, purifying compounds, and drying samples. While traditional evaporation relies on heat to remove solvents, evaporation under vacuum offers a more efficient and versatile approach. By reducing the pressure, vacuum evaporation lowers the boiling point of solvents, allowing for faster and safer evaporation at lower temperatures. This article explores when and why evaporation under vacuum is helpful, highlighting its advantages, applications, and key considerations.<h3>Understanding Evaporation Under Vacuum</h3>Evaporation under vacuum, also known as vacuum evaporation, involves reducing the atmospheric pressure around a liquid, which decreases its boiling point. This allows the solvent to evaporate at a lower temperature than it would under normal atmospheric conditions. The process typically employs equipment like rotary evaporators and vacuum ovens, which create a controlled low-pressure environment to facilitate efficient solvent removal.<h4>How It Works:</h4><ul><li>Pressure Reduction:&nbsp;A vacuum pump reduces the pressure in the system.&nbsp;</li><li>Lower Boiling Point:&nbsp;The reduced pressure lowers the boiling point of the solvent.&nbsp;</li><li>Evaporation:&nbsp;The solvent evaporates at the lower temperature, leaving behind the concentrated sample or dried product.</li></ul><h3>Advantages of Vacuum Evaporation&nbsp;&nbsp;</h3><h4>Enhanced Efficiency and Speed&nbsp;</h4>Vacuum evaporation significantly speeds up the solvent removal process. The lower boiling point means that solvents evaporate more quickly, reducing the time required for concentration or drying.<h4>Lower Temperatures</h4>Evaporating at lower temperatures is crucial for preserving thermally sensitive compounds that might degrade under higher heat. This is particularly important in pharmaceutical and biochemical applications.<h4>Improved Safety&nbsp;</h4>By avoiding high temperatures, vacuum evaporation reduces the risk of thermal decomposition and hazardous reactions. It also minimizes the potential for solvent vapors to become flammable or explosive.<h4>Reduced Solvent Usage and Waste&nbsp;</h4>Vacuum evaporation often requires less solvent and generates less waste. This is beneficial for both cost savings and environmental sustainability. For example, Organomation <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products?category=338&amp;distributorItems=332&amp;search=evap">large scale evaporators</a> are capable of recollecting up to 97% of starting solvent.<h3>Applications in Laboratory Settings&nbsp;</h3><h4>Sample Concentration&nbsp;</h4>Vacuum evaporation is widely used to concentrate samples for analytical techniques such as <a target="_blank" rel="noopener noreferrer" href="https://www.organomation.com/hplc-sample-preparation">high-performance liquid chromatography</a> (HPLC) and <a target="_blank" rel="noopener noreferrer" href="https://www.organomation.com/preparing-samples-for-gc-ms/ms-analysis">gas chromatography-mass spectrometry</a> (GC-MS). Concentrating the sample improves the detection limits and accuracy of these methods.<h4>Drying Samples</h4>It is also employed for drying samples before further analysis or storage. Removing moisture is crucial for accurate weight measurements and preventing degradation of sensitive compounds.<h4>Preparation for Crystallization&nbsp;</h4>In crystallization studies, vacuum evaporation can be used to concentrate solutions to supersaturation, facilitating the formation of crystals.<h3>Industrial Applications of Vacuum Evaporation&nbsp;</h3><h4>Environmental Analysis&nbsp;</h4>In environmental labs, vacuum evaporation concentrates pollutants from large volume water samples, allowing for more accurate detection and quantification of contaminants<h4>Chemical Manufacturing&nbsp;</h4>Vacuum evaporation is employed in chemical manufacturing for solvent recovery and recycling, reducing costs and environmental impact.<h4>Pharmaceutical Industry&nbsp;</h4>In pharmaceutical manufacturing, vacuum evaporation is essential for purifying active pharmaceutical ingredients (APIs) by removing solvents and other impurities without degrading the product.<h4>Food and Beverage Industry&nbsp;</h4>The food industry uses vacuum evaporation to concentrate flavors and extracts. This process enhances the intensity of flavors while preserving the quality of the ingredients.<h3>Key Considerations for Vacuum Evaporation&nbsp;</h3><h4>Equipment Selection</h4>Choosing the right equipment is crucial for successful vacuum evaporation. The selection depends on the sample type, volume, and specific application requirements. Here are the main types of evaporators that integrate vacuum:Rotary evaporators: Rotary evaporators, commonly referred to as "rotovaps," are widely used in laboratories for efficiently removing solvents from samples. They consist of a rotating flask, a condenser, and a vacuum system. The rotating motion increases the surface area for evaporation, and the vacuum reduces the boiling point of the solvent, making the process faster and more efficient.Large Scale Parallel Evaporators: <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products?category=338&amp;distributorItems=332&amp;search=evap">Organomation S-EVAP</a> is a specialized evaporator designed for the efficient concentration of multiple samples simultaneously. The optional vacuum manifold system to reduce the boiling point of solvents, facilitating faster evaporation at lower temperatures. This system is ideal for laboratories needing to concentrate samples in Kuderna-Danish (KD) flasks, often used in environmental testing, food and beverage analysis, and pharmaceutical research. The S-EVAP provides precise control over temperature and vacuum levels, ensuring reproducibility and safety in sample processing.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Organomation_S_EVAP_RB_Solvent_Evaporator_10_position_48376ce49a.jpg" alt="Organomation: When is Evaporation Under Vacuum Helpful?: Organomation S-EVAP-RB Solvent Evaporator - 10 position." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Organomation_S_EVAP_RB_Solvent_Evaporator_10_position_48376ce49a.jpg 120w," sizes="100vw" width="430" height="560">Vacuum ovens: Vacuum ovens are used for drying samples that are sensitive to heat or require low-temperature evaporation. They provide a controlled environment where the pressure and temperature can be precisely adjusted. Vacuum ovens are ideal for drying solid and viscous samples, as well as for performing vacuum distillations.Centrifugal evaporators: Centrifugal evaporators use a combination of vacuum, heat, and centrifugal force to evaporate solvents. They are particularly useful for high-throughput applications where multiple samples need to be processed simultaneously. These systems are commonly used in drug discovery and biochemical research.<blockquote>Discover: <a target="_blank" rel="noopener noreferrer" href="https://blog.organomation.com/blog/when-nitrogen-blowdown-is-preferable-over-centrifugal-evaporation">When Nitrogen Blowdown is Preferable Over Centrifugal Evaporation</a></blockquote>Falling film evaporators: Falling film evaporators are used for continuous evaporation processes, where the liquid flows down a heated surface in a thin film. The vacuum system reduces the boiling point, and the thin film facilitates rapid solvent evaporation. These evaporators are used in large-scale industrial applications, such as in the food and beverage industry.Freeze dryers: Freeze dryers, or lyophilizers, integrate vacuum to sublimate frozen solvents directly from the solid to the gas phase. This technique is used for drying thermally sensitive materials, such as biological samples and pharmaceuticals, without damaging their structure or activity.<blockquote>Discover: <a target="_blank" rel="noopener noreferrer" href="https://blog.organomation.com/blog/how-does-nitrogen-blow-down-compare-to-lyophilization">How Nitrogen Blow Down Compares to Lyophilization</a></blockquote>Spray dryers: Spray dryers use a vacuum system in combination with a spray mechanism to evaporate solvents from liquid samples. The liquid is atomized into fine droplets, which are then exposed to a heated gas stream under vacuum, causing rapid solvent evaporation. This method is used for producing powders and granules from liquid solutions.<h4>Solvent Properties</h4>Understanding the properties of the solvents being used is essential. Different solvents behave differently under vacuum, and their boiling points, vapor pressures, and potential for forming azeotropes must be considered.Vacuum evaporators excel in processing samples with naturally high boiling points, such as dimethyl sulfoxide (DMSO), N,N-dimethylformamide (DMF), and water. The reduced pressure lowers the boiling points, making the evaporation process more efficient and less thermally stressful for sensitive samples.Understanding how solvents behave under reduced pressure, including potential azeotrope formation, is critical for effective evaporation.<h4>Process Control&nbsp;</h4>Monitoring and controlling temperature and pressure are vital for optimizing the evaporation process. Precise control ensures efficient solvent removal while protecting the sample from degradation.<h4>Safety Precautions</h4>Proper handling of volatile and hazardous solvents is necessary to prevent accidents. This includes using appropriate containment, ventilation, and personal protective equipment.Evaporation under vacuum is a powerful and versatile technique with numerous advantages over traditional evaporation methods. It offers enhanced efficiency, lower operating temperatures, and improved safety, making it invaluable in both laboratory and industrial settings. As technology advances and new applications arise, the role of vacuum evaporation will continue to expand, driving innovation and improving outcomes across various scientific and industrial fields.<blockquote>To find out the best evaporation method for your needs, start a conversation with our experts at <a href="mailto:sales@organomation.com">sales@organomation.com</a>, or use our handy <a target="_blank" rel="noopener noreferrer" href="https://www.organomation.com/evaporation-method-recommendation-tool">evaporation method recommendation tool</a>.</blockquote>

When is Evaporation Under Vacuum Helpful?

🎤 Presenter: Masaaki Ubukata (Tokyo, Akishima, Japan)💾 <a target="_blank" rel="noopener noreferrer" href="https://gcms.cz/paper/28901">PDF presentation</a><blockquote>💡 Book in your calendar: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/events/787">17th Multidimensional Chromatography Workshop (MDCW)</a> 13 - 15. January 2026</blockquote><h3>Abstract</h3>GC-MS plays an important role in a lot of application fields and is widely used for qualitative and quantitative analysis, especially for volatile organic compounds. Most of the qualitative analysis in GC-MS is compound identification by comparison with commercially available library databases for the EI mass spectra. The EI mass spectral pattern, which is commonly used in GC-MS, is known to be highly reproducible and independent of the instrument. Therefore, a large number of EI mass spectra are available in commercial databases, and it becomes an advantage comparing with qualitative analysis in LC-MS.However, there are still many compounds that are not registered in commercial EI mass spectral databases. For this qualitative analysis issue, we have created an AI model to predict EI mass spectra from structural formulas by machine learning.We prepared approximately 100 million compounds structures from PubChem, 10 million TMS compounds and 5.5 million pyrolyzates compounds using in-silico. Totally, we have created a new predictive EI mass spectral database for 120 million compounds that are not registered in commercial databases.In this study, we report the details of the development for the predicted EI mass spectral database and applying to comprehensive 2-dimentional gas chromatography data.

Unknown compounds analysis by HRMS, soft ionization and AI for GCxGC (Masaaki Ubukata, MDCW 2025)

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 12th May 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">LabRulezICPMS</a> libraries.</blockquote>This week we bring you technical note by Agilent Technologies, application note by Shimadzu and poster by MDCW!<h3>1. Agilent Technologies: How Does Bleed Impact GC/MS Data and How Can It Be Controlled?</h3><ul><li>Technical note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/te_bleed_impact_gc_ms_data_5994_7586en_agilent_1_728100a153.pdf">Full PDF for download</a></li></ul><h4>Understanding column bleed&nbsp;</h4>Column bleed remains one of the most commonly observed yet misunderstood aspects of mass spectrometry (MS) data. Bleed elevates chromatographic baselines and creates spectral interference, lowering the quality of and confidence in your data. To understand bleed, it must first be considered where the bleed originates. While columns come in a wide variety of phase types, the most commonly used columns today, such as the 1, 5, and 624, are categorized as wall-coated open tubular (WCOT) columns. These columns are composed of fused silica tubing (with varying internal diameters, measured in mm), internally coated with a thin film of stationary phase (with varying thicknesses, measured in μm), as shown in Figure 1. This coated stationary phase interacts with analytes and creates the selectivity and retention characteristics of the chromatography; but, these same characteristics are the origins of column bleed.Column phases can be made from a wide variety of polarities of liquid polymers with a polysiloxane backbone. When heat is applied, the terminal end of the stationary phase polymer starts to bend back and attack itself, which is called "backbiting." Ring structures, which are thermodynamically stable, become liberated and increase the noise and raise the baseline, as shown in Figure 2. The process is then repeated. The higher the temperature provided, the faster the reaction is driven, which is why there is an increase in baseline at temperatures above 300 °C.&nbsp;An increase in the rise of a baseline can be problematic for low signal-to-noise analytes, as peak integration can negatively impact data quality. Stable, flat baselines optimize the accuracy and repeatability of peak integration. When working with sensitive detectors, such as MS, an increase in the sensitivity of the detector also increases the background noise and bleed detection, causing excess column bleed to be detrimental to the sensitivity of trace level compounds.<h4>Experimental</h4>An Agilent<a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=+8890+GC"> 8890 GC</a> coupled with a flame ionization detector (FID), and an Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=5977B+GC%2FMSD+">5977 Series B GC/MSD </a>were used to collect data. Data acquisition was performed using Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=OpenLab+ChemStation">OpenLab ChemStation</a> and <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=MassHunter+acquisition+software">MassHunter acquisition software</a>. Additionally, an Agilent <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=Intuvo+9000+GC">Intuvo 9000 GC</a> coupled with an FID was used to collect data. <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?manufacturerItems=1&amp;search=J%26W+DB-5Q">J&amp;W DB-5Q and J&amp;W&nbsp;HP‑5Q GC columns </a>were compared to various conventional, commercially available 5ms GC columns.<h4>Results and discussion&nbsp;</h4><h5>Comparisons of bleed profiles at upper temperature&nbsp;limits&nbsp;</h5>To compare the thermal stability of the HP-5Q columns to conventional 5ms columns, columns were installed on an 8890 GC equipped with dual split/splitless inlets and dual FIDs, and experiments were done in tandem. After confirming that column connections were properly installed, free of leaks, and conditioned, the oven temperature was ramped up to temperatures of 330 and 340&nbsp;°C and held for 10 minutes each. Then, the oven temperature was ramped to a final temperature of 350&nbsp;°C (the programed MAOT of the column phases) and held for 30 minutes. As shown in Figure&nbsp;4, both the DB-5Q and HP-5Q maintained ultralow FID response at the upper temperature limits, both maintaining column bleed levels below 1.0 pA at 340 °C. Also, when operating the columns at 350 °C (the programmed maximum temperature) over a period of 10 hours, both the DB-5Q and HP-5Q maintained bleed levels below 2.0 pA, while the conventional 5ms columns X and Y had bleed levels at 10 and 4 pA respectively, demonstrating the increased thermal stability of the DB-5Q and HP-5Q GC columns.<h4>Conclusion&nbsp;</h4>While column bleed is a normal phenomenon, there are ways to decrease its impact on the analysis and sensitivity of the detector being used. Improved column technology, with the introduction of the Agilent J&amp;W DB-5Q and HP-5Q GC columns, has provided an increase in thermal stability that dramatically reduces column bleed. The decrease in column bleed at high temperatures allows an increase in sensitivity of mass spectrometers, as the spectral interference from ions due to backbiting of column phase is reduced. This demonstrates that the DB-5Q and HP-5Q GC columns are optimal for use with sensitive detectors such as GC/MS, triple quadrupole GC/MS, and GC/Q-TOF.<h3>2. MDCW: Group-type quantitation of hydrocarbons in aviation fuel using GC×GC–FID&nbsp;</h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/2025_001_MDCW_ASTM_D8396_9a3aa6f3e5.pdf">Full PDF for download</a></li></ul>Accurate hydrocarbon composition of finished fuels, such as aviation fuel, is required to ensure quality control and to determine the effects of processes in fuel production. This has become even more important with the development of novel renewable fuels, such as sustainable aviation fuels (SAFs).Here, we demonstrate the use of reverse fill/flush (RFF) flow-modulated GC×GC–FID and automated group-type data processing to provide fast and accurate quantitative information on hydrocarbon composition.<h4>Experimental</h4><ul><li>Samples: A reference standard and reference blends of both diesel and aviation turbine fuel.&nbsp;</li><li>GC×GC: Modulator: INSIGHT®-Flow reverse fill/flush (RFF) flow modulator (SepSolve Analytical); Modulation period (PM): 7.8 s. Carrier gas: H2.&nbsp;</li><li>Column set: ASTM D8396 reverse phase column set (SepSolve Analytical, PN: OEM-SEP-COLKIT-10)&nbsp;</li><li>FID: Total H2 flow (column &amp; fuel): 50 mL/min; Air flow: 350 mL/min: Makeup gas flow: 5 mL/min; Temperature: 300 °C.&nbsp;</li><li>Software: <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?search=ChromSpace%C2%AE+GC%C3%97GC+software">ChromSpace® GC×GC software</a> for instrument control and data processing</li></ul><h4>Results and discussion</h4><h5>Optimising the GC×GC separation&nbsp;</h5>Separation was optimised using a custom column set and larger loop volume, enabling excellent separation of the key chemical classes (Figure 2).The INSIGHT-Flow modulator used in this study has an adjustable sample loop (in the range of 25-250 μL) for greater flexibility in method development. The reference standard was analysed in replicate (n=10) to assess method repeatability and precision. The relative standard deviation (RSD) of the raw peak areas were all &lt;2%, while the calculated mass percent values were consistently within 0.5% of the known composition.&nbsp;<h5>Group-type classifications&nbsp;</h5>Group-type analysis of these key chemical classes was then performed on various fuels using the ‘stencil’ workflow in ChromSpace software (Figure 3). Once a stencil is created, it can be saved and applied to multiple data files in an automated batch sequence to generate area percent reports. This means that the method is then scalable across multiple GC×GC–FID platforms for fast classification. This proven workflow has already gained accredited status in a number of high-throughput environmental labs for the analysis of total petroleum hydrocarbons (TPH).<h4>Conclusions</h4>This poster has shown an end-to-end workflow for ASTM Method D8396, specifically:&nbsp;<ul><li>Proven reverse fill/flush modulation using the INSIGHT-Flow, a modulator in operation in numerous high-throughput labs across the world.&nbsp;</li><li>Optimal class separation with a tried-and-tested column set.&nbsp;</li><li>Fast, straightforward group-type data processing with ChromSpace software.&nbsp;</li><li>Doubled productivity with optional dual-channel GC×GC technology.&nbsp;</li><li>A retrofittable solution for all popular GCs, allowing existing systems to be upgraded to GC×GC capability</li></ul><h3>3. Shimadzu: Analysis of Dechlorane Plus Residues in Environmental Water Using <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-TQ8050+NX">GCMS-TQ8050 NX</a> with Boosted Efficiency Ion Source(BEIS) and Long-Life Filament</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_03_gcmsms_566_en_93e41bdffc.pdf">Full PDF for download</a></li></ul>User Benefits:<ul><li>The combination of the BEIS and long-life filament enables high sensitivity analysis while maintaining long-term stability.</li><li>The 13C-Dechlorane 602 is used as internal standard(IS) in the optimization method to avoid the interference of isotope IS with target components in MRM mode.</li></ul>Dechlorane Plus (DP) is a synthetic substance mainly used as an adhesive, sealant and flame retardant for polymers in the industrial field. Due to its strong persistence and bioaccumulation, there is a significant risk to human and environmental health. In 2018, the European Chemicals Agency (ECHA) identified it as a Substance of Very High Concern (SVHC), and in June 2021 proposed to add it to Appendix XVII of the REACH regulation to restrict it, proposing to ban the production and use of DPs and prohibit the production and launch on the market of goods with DP content equal to or greater than 0.1% (by weight). In May 2023, the Stockholm Convention on Persistent Organic Pollutants (POPs) listed DP in Appendix A. At the same time, DP is also included in China's List of new pollutants under Key Control (2023 version).&nbsp;A method for the determination of residues of DPs in environmental water was established by using the Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library?mainauthorItems=1&amp;search=GCMS-TQ8050+NX">GCMS-TQ8050 NX</a> equipped with Boost Efficiency Ion Source and long-life filament. This application news provides an important analytical method for determine the residue levels of new pollutantsin environment with high sensitivity and good stability.<h4>Quantitative Analysis</h4>In the initial scheme, 13C-DP was used as the IS. However, due to the same retention time of 13C-DP and the target compound, the characteristic ions cause interference, resulting in a large calibration curve intercept and a high RF RSD (&gt;80%). Therefore, 13C-Dechlorane 602 is used as the IS instead. Its retention time differsfrom target DP, which helps avoid the interference.<h4>Evaluation of Durability in Analysis of Standard Solution and Samples</h4>The sample solution and 0.5 ng/mL standard solution were tested to evaluate the long-term durability of response. A total of 500 analyses of the sample and 80 analyses of standard solution were conducted. Fig.3 shows the durability test results of the standard solution. The horizontal axis shows the number of analyses, while the vertical axis shows the peak area ratio for each analysis number. The results indicate that the changes in peak area ratio and ion proportion were within ±20% of the average value (calculated from very beginning 20 injections).<h4>Conclusion</h4>A method for the determination of DP residues in environmental water was established by using the Shimadzu GCMS-TQ8050 NX combined with BEIS and long-life filament. The target compound exhibited good linearity in the concentration range of 0.2 to 50.0 ng/mL and the RF RSD of calibration curve was less than 15 %. The standard solution of 0.2 ng/mL was injected for 10 consecutive times to measure the LOD with results of 0.063 and 0.103 ng/mL. The durability of DP response was investigated by alternating test of sample solution and standard solution, and the peak area ratio in standard solution fluctuated within 20% in 500 injection of samples. The recovery rate of 1 ng/mL in blank samples was around 102 %. The method has high sensitivity and good repeatability and is suitable for the determination of DP residues in surface water, groundwater, industrial wastewater, and domestic sewage.

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When is Evaporation Under Vacuum Helpful?

News from LabRulezGCMS Library - Week 20, 2025

Unknown compounds analysis by HRMS, soft ionization and AI for GCxGC (Masaaki Ubukata, MDCW 2025)